色谱 ›› 2017, Vol. 35 ›› Issue (7): 748-754.DOI: 10.3724/SP.J.1123.2017.03040

• 研究论文 • 上一篇    下一篇

高效液相色谱-荧光检测法测定橄榄油中4种多环芳烃

赵佳莹1,2, 李晓敏2, 卢晓华2, 张庆合2, 张维冰1   

  1. 1. 齐齐哈尔大学化学与化学工程学院, 黑龙江 齐齐哈尔 161006;
    2. 中国计量科学研究院化学计量与分析科学研究所, 北京 100029
  • 收稿日期:2017-03-29 出版日期:2017-07-08 发布日期:2013-10-18
  • 通讯作者: 李晓敏,Tel:(010)64524784,E-mail:lixm@nim.ac.cn;张维冰Tel:(021)64252145,E-mail:weibingzhang@ecust.edu.cn
  • 基金资助:

    国家重点研发计划资助项目(2016YFF0201106).

Determination of four polycyclic aromatic hydrocarbons in olive oil by high performance liquid chromatography-fluorescent detection

ZHAO Jiaying1,2, LI Xiaomin2, LU Xiaohua2, ZHANG Qinghe2, ZHANG Weibing1   

  1. 1. College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China;
    2. Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China
  • Received:2017-03-29 Online:2017-07-08 Published:2013-10-18
  • Supported by:

    National Key Research and Development Program of China (No.2016YFF0201106).

摘要:

建立了高效液相色谱-荧光检测(HPLC-FLD)测定橄榄油中苯并[a]蒽、屈、苯并[b]荧蒽、苯并[a]芘4种多环芳烃(PAHs)的分析方法。橄榄油样品经异丙醇稀释,采用具有 π-π 特异性作用的固相萃取柱净化,Agilent ZORBAX Eclipse PAH色谱柱(100 mm×2.1 mm,1.8 μ m)分离,以水-乙腈为流动相,梯度洗脱,实现了4种化合物的基线分离,并用基质匹配校准溶液进行外标法定量。4种多环芳烃的线性范围为2.4~40 μ g/L,相关系数(r)为0.9990~0.9999,方法的定量限为0.147~0.413 μ g/L,加标回收率为95.5%~103.2%,日内和日间精密度(RSD)分别为0.10%~1.69%和2.48%~2.93%(n=5)。该法具有灵敏度高、检出限低、重复性好等特点,适用于橄榄油中4种PAHs快速、准确的定量检测。

关键词: 多环芳烃, 橄榄油, 高效液相色谱-荧光检测法, 固相萃取

Abstract:

A method for the determination of four polycyclic aromatic hydrocarbons (PAHs) such as benzo[a]anthracene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene in olive oil by high performance liquid chromatography-fluorescent detection (HPLC-FLD) was developed. The olive oil samples were diluted with isopropanol and cleaned-up by a solid phase extraction cartridge with π-π specificity. Critical isomers were separated by gradient elution with water-acetonitrile on an Agilent ZORBAX Eclipse PAH column (100 mm×2.1 mm, 1.8 μ m). The calibration was performed by the use of matrix-matched calibration standards. The results showed that there were good linear relationships for the four PAHs in the range of 2.4-40 μ g/L with correlation coefficients of 0.9990-0.9999. The limits of quantification (LOQs) ranged from 0.147 to 0.413 μ g/L, and the recoveries of the spiked samples ranged from 95.5% to 103.2%. The intra-day and inter-day precisions were in the ranges of 0.10%-1.69% and 2.48%-2.93% (n=5), respectively. The method has the characteristics of high sensitivity, low detection limit and good precision, and is suitable for rapid and accurate quantitative detection of the four PAHs in olive oil.

Key words: high performance liquid chromatography-fluorescent detection (HPLC-FLD), olive oil, polycyclic aromatic hydrocarbons (PAHs), solid phase extraction (SPE)

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